Surface Energy Analyser -

Surface Energy Analyser -

Surface Energy Analyser Application Science Team Surface Measurement Systems January 2016 Agenda Inverse Gas chromatography technique Concept Principle Surface Energy Analyser (SEA) Introduction Properties measured by the Instrument Competitors Overview Applications/Markets Summary Conclusions Surface Energy Analyser by SMS.

Based on the Inverse Gas chromatography technique (IGC) What is IGC? IGC History First publication discussing the technique dates from earlies 80s. Nowadays, hundreds of publications about surface energy of polymers, catalyst, fibres, composites, APIs, etc can be found across different journals. Almost the all early studies used a home-build iGC. - None produced iGC that time. Since the invention of the Surface Energy Analyser (SEA), the IGC technique became commercially accessible in the form of an automated and fully controllable system Latest published SEA papers Composite - Powder Technology 270 (2015) 112120 Food - Food Chemistry 174 (2015) 2530 Zeolite - Journal of Chromatography A, 1362 (2014) 250261

Pharma - Pharm Res (2015) 32:248259 Introduction Inverse Gas Chromatography (IGC) principles*: 1st developed in 1950s. Inverse gas chromatography (IGC) is a versatile, powerful, sensitive and relatively fast technique for characterizing the physicochemical properties of materials. Due to its applicability in determining surface properties of solids in any form such as films, fibres and powders of both crystalline and amorphous structures, IGC became a popular technique for surface characterization IGC Concept Mobile phase: Unknown Gas/Vapors Mobile phase Known Gas/Vapor

Stationary phase: Known solid (Generally provided by Instrument Manufacturer) Stationary phase: Unknown solid. (Sample to characterize) Animation by L. Teng, Surface Measurement Systems iGC Principle Pack a column with the sample of interest Select probes Non-polar solvent for the dispersive interaction Polar solvents for the specific interactions Inject them at infinite and/or finite dilution

From the retention time the different physicochemical properties can be determined iGC Principle cont. Pack a column with the sample of interest Sample Silane-treated glass tube 30cm long & 6 mm O.D. 2, 3 & 4 mm I.D. 10 mg 500 mg of material typically 0.5 m2 of surface area Glass wool

iGC Principle cont. Select probes Non-polar solvent for the dispersive interaction Polar solvents for the specific interactions New injection scheme: *1:4000 Injection Ratio * Controlled by injection pulse (15ms 60,000ms) * Allows wider range of concentrations * Allows exact dosing of number of probe molecules 12 solvent reservoirs (2 drawers of 6 reservoirs each) Easy access drawers

Temperature-controlled for vapor stability Fully automatic up to 2500 injections in a sequence iGC Principle cont. Decane Nonane Inject them at infinite and/or finite dilution Octane Heptane 30% 60% 70% 75%

Surface Coverage IGC Principle: Retention Time Detector response t0 tR,Hexane tR,Heptane tR,Octane From the retention time the different physicochemical properties can be determined Methane

Hexane Heptane Octane Time Single pulse of probe molecule t0 is the retention time for an inert molecule (distribution coefficient KR = 0, CH4, Ar, N2 & H2)

tR is the retention time for the interacting probe Net retention time tN = tR - t0 Surface Energy Analyser by SMS. What is the SEA and what are the instrument specs? SEA Introduction Our Surface Energy Analyser is the new generation of the inverse Gas Chromatography technique. It is specially designed to determine the surface energy heterogeneity but nevertheless suitable to measure different surface and bulk properties of solid materials such

as Adsorption isotherms, Heat of sorption, Glass Transition Temperature, Solubility Parameters and so on. Compact design Small footprint: 450 mm (18) x 450 mm (18) x 700 mm (27.5) 12 vapor reservoirs (50 ml) 2 column oven design: 20 to 150 C Flame Ionization Detector (FID) User Friendly Control and Analysis Software Safety Features: Hydrogen Leak & Organic Vapor Leak Detectors SEA Variable Injection Scheme

Solvent pulse sizes of greatest precision and range Reproducibility of iGC SEA Instrument-to-Instrument: RSD 0.69% (n>10) Experiment-to-Experiment: RSD 1.20% (n>10) Column-to-Column: RSD 1.00% hexane Additional Features *Background Humidity Control: 0 to 90% RH (at 25 C) Allows to run the experiments under real conditions *Film Cell external bench-top unit Surface of film or plate can be measured with this accessory Surface Energy Analyser by SMS.

What properties can be measured by SEA? Properties measured by SEA Surface Energy Analysis Dispersive, acid-base components & total surface energy Knowledge of surface energetics is Acid-base Free Energy of Desorption Analysis important Heterogeneity Mapping

design of multi-component systems Heterogeneity profiles, heterogeneity distributions Gutmann Acid/Base Properties Isotherm Analysis Peak Max, ECP tailing & fronting, Henrys constant BET Specific Surface Area Thermodynamic Work of Adhesion/Work of Cohesion Heat of Sorption Bulk Solid Properties Glass Transition Temperature Solubility Parameter (Hildebrand 1D, Hansen 3D) Cross-linking Density in the

formulation and the prediction of processing performance. The surface energy heterogeneity profile constitutes an energy map of the material surface and also allows prediction of product properties, in particular in formulation of blends, composites or coatings What Does Surface Energy Affect? Surface Treatment effects on Surface Energy Investigation the influence of the surface treatment

Modifying surface energy of different materials at will Waxing, coating, silylation, hydrogenation, adsorption, relaxation High SE Low SE oxygen plasma treatment, chemical etching, sand blasting Surface Energy Analyser by SMS. Direct and Indirect competition Competition: overview

Direct Competitors None. The only manufacturers making an automated IGC system Indirect Competitors (other techniques) Home built IGC systems (modifying a Gas chromatographer) Contact Angle technique Atomic force Microscopy

Wetting Balance Surface Energy Analyser by SMS. Industry, Market and common applications Pharmaceutical Market/Applications Formulation or pre-formulation groups at large pharma companies Inhalation Powder properties extremely important to product performance Dedicated Inhalation drug delivery companies or inhalation groups within large pharma companies

Materials Characterization Groups or Physical Properties Groups University Physical Pharmacy Groups 23 Pharmaceutical Market/Applications Process-induced disorder Affects of milling/grinding/micronization Amorphous versus crystalline Product stability

Energetic heterogeneity Drug-Excipient Interactions Works of Adhesion/Cohesion Powder mixing/segregation/powder flow Polymorph Characterization Material properties Surface acidity-basicity Surface modification 24

Composites-Filler Market/ Applications Carbon Fibers Aerospace, automotive, carbon fiber manufacturers National/Government labs Research institutes/universities Natural Fibers Research institutes/universities Wood Composites Research institutes/universities Forestry Government labs Nanotechnology Nanocarbons, nanoclays, nano-cellulose Research institutes/universities

National/government labs 25 Composites-Filler Market/ Applications Works of Adhesion/Cohesion Use surface energy to predict and measure interaction between two surfaces Surface Modification/Characterization Chemical change surface groups to make surface more compatible Long-term stability of surface groups Aging of surface treatments Effectiveness of surface coatings

26 Polymer Market/Applications Large, multi-national chemical companies i.e. Dow, DuPont, BASF Most likely central analytic groups Specialty polymer companies Drug delivery groups/companies

Paint and coating companies 27 Polymer Market/Applications Glass transition temperatures Solubility parameters

Controlled release applications Polymer blends; penetration of dyes; supercritical fluids Degree of Crosslink True surface Tg Tg as a function of RH Drug eluting stents; controlled release applications

Curing of epoxies Surface Energy Composites works of adhesion/cohesion Coatings/Surface modification: chemical; mechanical; plasma Wood, fiber, nanofiller composites 28 Filtration Market/Applications Large Filtration companies Large Tobacco companies Defence labs/National labs

Personal protection groups Chemical warfare groups University research groups Membranes Selective filtration 29 Filtration Market/Applications Selective Filtration Tailor surface chemistry/structure to preferentially adsorb/interact with one species over another Tobacco

Filter unwanted chemical species (i.e. Carcinogens) and not flavor Chemical Agents Detect chemical warfare agents Soldier and equipment protection from chemical warfare agents 30 Surface Energy Analyser by SMS. Summary

iGC-SEA Sales Points Hardware 2 column position oven design - two samples can be prepared and can be run sequentially, automatically No need for separate outgassing facilities, since this will be achieved by conditioning the sample in-situ by purging column with inert carrier gas Easier column packing procedure due to the column is straight (compared to some home-built systems)

Precise and wide range of injectable amounts vapor phase injection not liquid (as with manual injections) iGC-SEA Sales Points Scientific Support Customer Education is Paramount Not always mainstream technique Sample demonstration is common Must make customer comfortable with the technique and data

Utilize SMS Application Science Team Unique Applications Only robust method to measure surface energy of powders, fibers, and particulates Unique capability of measuring energetic heterogeneity of materials Few techniques can actually determine solubility parameters (computational methods most commonly used)

SMS World Leaders in IGC Theory, Instrumentation, and Applications Dedicated IGC Applications Specialists Two dedicated applications laboratories Authors and co-authors on several peer-review journal articles per year SMS presents research at several international meetings

Scientific support for lifetime of instrument 33 Conclusion s SEA a versatile and sensitive gas phase sorption technique for the physicochemical characterization tool for powders, fibers, films, particulates, semisolids SMS are innovators and market leaders in the realm of Inverse Gas Chromatography applications and science. More information on specific applications can be obtained by emailing [email protected] .

Head Office: United States Office: Surface Measurement Systems, Surface Ltd. Measurement Systems, Ltd, NA 5 Wharfside, Rosemont Road 2125 28th Street SW, Suite 1 London HA0 4PE, UK Allentown PA, 18103 Tel: +44 (0)20 8795 9400 Tel: +1 610 798 8299 Fax: +44 (0)20 8795 9401 Fax: +1 610 798 0334 Email: [email protected]

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